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Preparation method of amphipathic catalyst TS-1@AOF

A TS-1, catalyst technology, applied in the field of petroleum additives, can solve the problems of complex process, high cost, harsh conditions, etc., and achieve the effect of simple process and cost saving

Active Publication Date: 2019-06-14
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has its obvious disadvantages: after the reaction is completed, these surfactants are often mixed in the product, making the further purification of the product more difficult and causing the production process to be more complicated.
In this method, after the synthesis of non-amphiphilic solid nanoparticles, the surface is modified with organic groups containing quaternary ammonium salts. The process is complicated, the conditions are harsh, and the cost is high.

Method used

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  • Preparation method of amphipathic catalyst TS-1@AOF
  • Preparation method of amphipathic catalyst TS-1@AOF
  • Preparation method of amphipathic catalyst TS-1@AOF

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1 Preparation of Amphiphilic Catalyst TS-1@AOF

[0036] This example provides a specific method for preparing the amphiphilic catalyst TS-1@AOF, comprising the following steps:

[0037] 1) Synthesis of titanium silicate molecular sieve TS-1

[0038] After mixing 8ml of TPAOH, 5ml of TEOS and 5ml of secondary water, stir at room temperature for 24 hours to form solution A; add 0.2mL of TBOT to 10.0mL of 30% H 2 o 2 , solution B was formed.

[0039]Solution B was added dropwise to solution A and stirred at room temperature for 24 hours to form a transparent sol. The formed transparent sol was put into a stainless steel kettle, stood at 100 degrees Celsius for 24 hours, stood at room temperature, centrifuged, washed twice with water, and washed once with alcohol. Calcined at 550°C for 6 hours to remove template TPA + .

[0040] 2) Synthesis of vinyl-modified TS-1

[0041] 0.10g TS-1 nanoparticles were sonicated in 50ml 0.1M HCl for 10 minutes, centrifuged, w...

Embodiment 2

[0046] Embodiment 2 catalytic activity verification

[0047] To demonstrate the superiority of the TS-1@AOF material, we conducted a control experiment. The comparative catalytic material is TS-1@PMO 1 and TS-1@PMO 2 Two kinds of nanoparticles with yolk-shell structure. PMO 1 The shell was prepared by hydrolysis and polymerization of the non-amphiphilic organosilane precursor BTOSVB, while PMO 2 The shell is prepared by hydrolysis and polymerization of the non-amphiphilic organosilane precursor BTEB. TS-1@PMO 1 and TS-1@PMO 2 The specific catalytic experimental process of the two egg yolk-shell nanoparticles is consistent with the traditional catalytic process of the Pickering catalytic process of TS-1@AOF amphiphilic solid nanoparticles.

[0048] Pickering catalytic process: 50mg of TS-1@AOF amphiphilic solid nanoparticles were added to 1.5ml of hydrogen peroxide solution (30wt%) and 1.5ml of 1-hexene, and sonicated for 15 minutes. At a temperature of 333K, let stand ...

Embodiment 3

[0052] Embodiment 3 catalytic scope

[0053] 50 mg of TS-1@AOF amphiphilic solid nanoparticles were added to solutions with 1-hexene / water ratios of 0.6, 0.8, 1.0, 1.2, and 1.4, and sonicated for 15 minutes. At a temperature of 333K, let stand to react for 1h.

[0054] The result is as figure 2 As shown, when the ratio of 1-hexene / water is 0.6, 0.8, 1.0, 1.2 and 1.4, their TON values ​​are 27.75, 27.7, 28.1, 27.9 and 27.8, respectively. It shows that the prepared amphiphilic TS-1@AOF nanoparticles are not only suitable for the 1-hexene / water ratio of 1:1, but also suitable for the catalytic reaction of other ratios of 1-hexene / water. And the TON value does not change much. TS-1@AOF has a wide range of applications, all of which can be attributed to the good amphiphilicity of the amphiphilic silicone skeleton AOF shell.

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Abstract

The invention discloses a preparation method of an amphipathic catalyst TS-1@AOF. The preparation method comprises the following steps: synthesizing a titanium-silicon molecular sieve TS-1; preparingvinyl-modified TS-1 / mSiO2 by using vinyl-modified TS-1 nanoparticles; coating TS-1@PS with polystyrene to obtain TS-1@mSiO2@PS; preparing mesoporous TS-1@PS@AOF nanoparticles with a core-shell structure; dissolving and extracting cetyltrimethyl ammonium bromide (CTAB) and polystyrene (PS) to obtain TS-1@AOF with a yolk-shell structure. The preparation process of an amphipathic shell is simple. Meanwhile, the selectivity and catalytic activity of 1,2-cyclohexane oxide are improved, and the cost is saved.

Description

technical field [0001] The invention belongs to the technical field of petroleum additives, and in particular relates to a preparation method of an amphiphilic catalyst TS-1@AOF. Background technique [0002] In today's organic synthesis and petrochemical reaction processes, some organic reagents are used as reaction solvents, such as methanol, acetonitrile and tetrahydrofuran. Most of these organic solvents are poisonous, pollute the environment and cost a lot. Water, as a non-polluting, cheap, and easy-to-obtain solvent, if it can be used as a substitute for organic solvents in organic synthesis and petrochemical reactions, its great significance to the entire human race is self-evident of. However, when water is used as a solvent, water and organic solvents are immiscible or have very little solubility, often forming a two-phase system with upper and lower layers. Due to the small contact area of ​​this two-phase system, the organic solvent contained in water will disso...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J35/02C07D303/04C07D301/12
Inventor 王润伟于洪豪
Owner JILIN UNIV
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